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液相色谱-串联质谱法测定人血浆中氯马斯汀的灵敏定量分析方法的建立与全面验证

Development and full validation of a sensitive quantitative assay for the determination of clemastine in human plasma by liquid chromatography-tandem mass spectrometry.

作者信息

Xie Zhiyong, Liao Qiongfeng, Li Zuojun, Zhu Chenchen, Zeng Yuaner, Liu Shikun

机构信息

Laboratory of Pharmaceutical Analysis & Quality Assessment, School of Pharmaceutical Sciences, Sun Yat-sen University, 74 Zhongshan Road II, Guangzhou 510080, China.

出版信息

J Pharm Biomed Anal. 2007 Aug 15;44(4):924-30. doi: 10.1016/j.jpba.2007.03.019. Epub 2007 Mar 27.

DOI:10.1016/j.jpba.2007.03.019
PMID:17475437
Abstract

A sensitive high-performance liquid chromatography-tandem mass spectrometry (LC/MS/MS) method was developed and validated for the determination of clemastine in human plasma. After having been extracted from plasma samples by ethyl acetate, clemastine and internal standard, diphenhydramine, were separated on a C(18) column. Detection was performed on Thermo Finnigan TSQ Quantum triple quadrupole mass spectrometer by selected reaction monitoring (SRM) mode via electrospray ionization (ESI) source. The method was linear in the concentration range of 5.0-1000.0 pg/ml for clemastine. The intra- and inter-day precisions were within 13.4% and the deviations were between -1.1% and 5.6%. The fully validated LC/ESI-MS/MS method has been successfully applied to the preliminary pharmacokinetic study in healthy male Chinese volunteers.

摘要

建立了一种灵敏的高效液相色谱-串联质谱(LC/MS/MS)法并进行验证,用于测定人血浆中的氯马斯汀。血浆样品经乙酸乙酯萃取后,氯马斯汀和内标苯海拉明在C(18)柱上分离。采用电喷雾电离(ESI)源,通过选择反应监测(SRM)模式在Thermo Finnigan TSQ Quantum三重四极杆质谱仪上进行检测。该方法在氯马斯汀浓度为5.0-1000.0 pg/ml范围内呈线性。日内和日间精密度均在13.4%以内,偏差在-1.1%至5.6%之间。该经过充分验证的LC/ESI-MS/MS方法已成功应用于中国健康男性志愿者的初步药代动力学研究。

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